CN111220657A - Polyacrylonitrile carbon fiber pH test method - Google Patents

Polyacrylonitrile carbon fiber pH test method Download PDF

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CN111220657A
CN111220657A CN202010228481.7A CN202010228481A CN111220657A CN 111220657 A CN111220657 A CN 111220657A CN 202010228481 A CN202010228481 A CN 202010228481A CN 111220657 A CN111220657 A CN 111220657A
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carbon fiber
deionized water
polyacrylonitrile carbon
polyacrylonitrile
electrode pen
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杨永岗
胡培贤
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Sinofibers Technology Co ltd
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Abstract

The invention belongs to the technical field of polyacrylonitrile carbon fiber performance test, and relates to a polyacrylonitrile carbon fiber pH test method, which comprises the steps of calibrating a pH electrode pen; weighing deionized water in a flask, adding polyacrylonitrile carbon fiber for mixing, arranging a condenser on the flask, then placing the flask in a heater, controlling the temperature of the deionized water in the flask, cooking the fiber, cooling, and keeping the cold deionized water and the polyacrylonitrile carbon fiber mixed solution for later use; and inserting the calibrated pH electrode pen into the cold deionized water and polyacrylonitrile carbon fiber mixed solution, and obtaining a test result as the pH value of the polyacrylonitrile carbon fiber after the test result is stable. The testing method is simple and accurate, and solves the problem that the pH value of the polyacrylonitrile carbon fiber can not be accurately tested at present.

Description

Polyacrylonitrile carbon fiber pH test method
Technical Field
The invention belongs to the technical field of polyacrylonitrile carbon fiber performance testing, and particularly relates to a polyacrylonitrile carbon fiber pH testing method.
Background
The polyacrylonitrile carbon fiber is a novel material with conductivity, high strength, low density, corrosion resistance and high temperature resistance, has limited flexibility, and can be woven, processed and wound for forming. The existing polyacrylonitrile carbon fiber production process has long route and many factors for imaging the carbon fiber performance, and the polymerization, spinning, oxidation, carbonization and post-treatment processes all have important influence on the performance of the polyacrylonitrile carbon fiber.
Therefore, mechanical property test, pH value test and the like of the polyacrylonitrile carbon fiber are one of important indexes for judging the polyacrylonitrile carbon fiber, and the prior art does not provide a test method for pH of the polyacrylonitrile carbon fiber.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects, the invention provides a simple and accurate method for testing the pH value of polyacrylonitrile carbon fiber, and solves the problem that the pH value of the polyacrylonitrile carbon fiber can not be accurately tested at present.
The technical scheme adopted by the invention for solving the technical problems is as follows: a polyacrylonitrile carbon fiber pH test method comprises the following steps:
s1, calibrating the pH electrode pen;
s2, pretreating polyacrylonitrile fibers: weighing deionized water in a flask, adding polyacrylonitrile carbon fiber for mixing, arranging a condenser on the flask, then placing the flask in a heater, controlling the temperature of the deionized water in the flask, cooking the fiber, cooling, and keeping the cold deionized water and the polyacrylonitrile carbon fiber mixed solution for later use;
s3, polyacrylonitrile fiber pH determination: inserting the pH electrode pen calibrated in the S1 into the mixed liquid of the cold deionized water and the polyacrylonitrile carbon fiber treated in the S2, and obtaining a test result of the pH value of the polyacrylonitrile carbon fiber after the test result is stable.
The method is used for measuring the pH value of the polyacrylonitrile carbon fiber, the polyacrylonitrile carbon fiber is boiled by using deionized water, and the pH value of the cooled mixed solution of the deionized water and the polyacrylonitrile carbon fiber is measured, so that the pH value of the polyacrylonitrile carbon fiber is obtained.
Further, the calibration of the S1pH electrode pen is specifically as follows:
s1-1, turning on a pH meter, and starting up to preheat for 10-30 min;
s1-2, taking out the pH electrode pen in the soak solution, washing the electrode pen with deionized water, and wiping the pH electrode pen clean with neutral filter paper;
s1-3, calibrating the pH electrode pen treated by the S1-2 in a buffer solution with the pH of 6.86 and the pH of 4, washing the calibrated pH electrode pen with deionized water, and wiping the pH electrode pen clean with neutral filter paper.
The pH electrode pen is calibrated, so that the change of asymmetric potential after the pH motor is practical for a period of time can be avoided, the pH electrode pen can accurately measure the pH value of the polyacrylonitrile carbon fiber after calibration, and the measurement error is avoided.
Further, the pretreatment of the polyacrylonitrile fiber S2 is specifically as follows:
s2-1, weighing 300 +/-0.2 g of deionized water, placing the deionized water in a 500mL round-bottom flask, adding a stirring magnetic rotor, and stirring the mixture on a stirrer;
s2-2, weighing wet polyacrylonitrile carbon fibers by 3m, and placing the polyacrylonitrile fibers in a round-bottom flask filled with deionized water;
s2-3, mounting a spherical condenser on the round-bottom flask, placing the round-bottom flask in a water bath heating pot, controlling the temperature of deionized water in the round-bottom flask to be 75 +/-2 ℃, cooking fibers, and keeping the cooking time for 30 min;
and S2-4, placing the round-bottom flask after the cooking is finished in a water bath at 25 +/-3 ℃ for cooling, and pouring 100mL of sample solution for later use when the temperature of the mixture of the deionized water and the polyacrylonitrile carbon fiber in the flask is reduced to 25 +/-3 ℃.
Through the polyacrylonitrile carbon fiber of a certain amount of deionized water and certain length that accurate control was weighed, the time of cooking is controlled, ensures that the deionized water dissolves the ion that is mingled with in the polyacrylonitrile carbon fiber in aqueous, and the temperature that the pH electrode pen measured temperature satisfies its standard survey, further improves the accuracy of polyacrylonitrile carbon fiber pH value measurement.
Furthermore, the soaking solution is saturated potassium chloride solution. The soaking solution can effectively protect the glass electrode at the front end of the pH electrode pen, so that the pH electrode pen can correspond well, and the asymmetric potential is greatly reduced and tends to be stable.
Further, the space between the S2-1 and the S2-2 also comprises S2-0, a pH electrode pen calibrated by the S1 is inserted into a round bottom flask of the S2-1 filled with deionized water, and the pH value of the deionized water is adjusted to 7.00 +/-0.03 by a pH adjusting liquid according to the measured value; the pH adjusting solution is 0.005mol/L sodium hydroxide solution or 0.005mol/L sulfuric acid solution. The deionized water filled in the round-bottom flask is calibrated, so that the measurement error caused by the deionized water is avoided, and the pH value of the polyacrylonitrile carbon fiber is accurate.
Further, when the wet polyacrylonitrile carbon fiber is measured by the S2-2 measuring device, the polyacrylonitrile carbon fiber is measured by the strand length measuring device in a state that the tension is 0, and when the fiber is cut, the polyacrylonitrile carbon fiber is in a tight state, and the cut is straight and neat. The stability that the polyacrylonitrile carbon fiber volume was got is controlled, and tension is 0, ensures that the accuracy of carbon fiber volume length is got, and control incision is straight, neat, has avoided the polyacrylonitrile carbon fiber to get the test error that causes, and the test is accurate.
Further, the pH meter used for calibrating the S1pH electrode pen is lightning PHS-3C.
The invention has the beneficial effects that:
1. the method is used for measuring the pH value of the polyacrylonitrile carbon fiber, the polyacrylonitrile carbon fiber is boiled by using deionized water, and the pH value of the cooled mixed solution of the deionized water and the polyacrylonitrile carbon fiber is measured, so that the pH value of the polyacrylonitrile carbon fiber is obtained.
2. The pH electrode pen is calibrated, so that the change of asymmetric potential after the pH motor is used for a period of time can be avoided, the calibrated pH electrode pen can accurately measure the pH value of the polyacrylonitrile carbon fiber, and the measurement error is avoided; through the polyacrylonitrile carbon fiber of a certain amount of deionized water and certain length that accurate control was weighed, the time of cooking is controlled, ensures that the deionized water dissolves the ion that is mingled with in the polyacrylonitrile carbon fiber in aqueous, and the temperature that the pH electrode pen measured temperature satisfies its standard survey, further improves the accuracy of polyacrylonitrile carbon fiber pH value measurement.
3. The soaking solution can effectively protect the glass electrode at the front end of the pH electrode pen, so that the pH electrode pen is ensured to correspond well, and meanwhile, the asymmetric potential is greatly reduced and tends to be stable; calibrating the deionized water filled in the round-bottom flask, so that the measurement error caused by the deionized water is avoided, and the pH value of the polyacrylonitrile carbon fiber is accurate; the stability that the polyacrylonitrile carbon fiber volume was got is controlled, and tension is 0, ensures that the accuracy of carbon fiber volume length is got, and control incision is straight, neat, has avoided the polyacrylonitrile carbon fiber to get the test error that causes, and the test is accurate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A polyacrylonitrile carbon fiber pH test method comprises the following steps:
s1, calibrating a pH electrode pen:
s1-1, turning on a pH meter which is thunder magnet PHS-3C, and starting up to preheat for 15 min;
s1-2, taking out the pH electrode pen soaked in the potassium chloride solution, washing the electrode pen with deionized water for 3 times, and wiping the pH electrode pen clean with neutral filter paper;
s1-3, calibrating the pH electrode pen treated by the S1-2 in a buffer solution with the pH of 6.86 and the pH of 4, washing the calibrated pH electrode pen with deionized water for 3 times, and wiping the pH electrode pen clean with neutral filter paper; the buffer solution with the pH value of 4 is a saturated solution of potassium hydrogen phthalate;
s2, pretreating polyacrylonitrile fibers:
s2-1, weighing 300.2g of deionized water on an electronic balance, placing the deionized water in a 500mL round-bottom flask, adding a stirring magnetic rotor, and stirring the mixture on a stirrer;
s2-0, inserting a pH electrode pen calibrated by S1 into the S2-1 round bottom flask filled with deionized water, and adjusting the pH value of the deionized water to 7.02 by using 0.005mol/L sodium hydroxide solution or 0.005mol/L sulfuric acid solution according to the measured value;
s2-2, measuring the wet polyacrylonitrile carbon fiber by using a filament yarn length measuring instrument in a state that the tension is 0, wherein the polyacrylonitrile carbon fiber is in a tight state when the fiber is cut off, the cut is straight and tidy, and the polyacrylonitrile fiber is placed in a round-bottom flask with the pH value of 7.02 deionized water;
s2-3, mounting a spherical condenser on the round-bottom flask, placing the round-bottom flask in a water bath heating pot, controlling the temperature of deionized water in the round-bottom flask to be 76 ℃, cooking fibers, and keeping the cooking time for 30 min;
s2-4, placing the cooked round-bottom flask in a water bath at 25 +/-3 ℃ for cooling, and pouring 100mL of sample solution for later use when the temperature of the mixed solution of deionized water and polyacrylonitrile carbon fibers in the flask is reduced to 25.5 ℃;
s3, polyacrylonitrile fiber pH determination: inserting the pH electrode pen calibrated in S1 into 100mL of deionized water and polyacrylonitrile carbon fiber mixed solution poured out after the treatment of S2, recording the pH value of the resin as 6.89 after the value shown by a pH meter is stable, wherein the value is the pH value of the polyacrylonitrile carbon fiber.
Example 2
A polyacrylonitrile carbon fiber pH test method comprises the following steps:
s1, calibrating a pH electrode pen:
s1-1, turning on a pH meter which is thunder magnet PHS-3C, and starting up to preheat for 15 min;
s1-2, taking out the pH electrode pen soaked in the potassium chloride solution, washing the electrode pen with deionized water for 3 times, and wiping the pH electrode pen clean with neutral filter paper;
s1-3, calibrating the pH electrode pen treated by the S1-2 in a buffer solution with the pH of 6.86 and the pH of 4, washing the calibrated pH electrode pen with deionized water for 3 times, wiping the pH electrode pen with neutral filter paper, wherein the buffer solution with the pH of 4 is a potassium hydrogen phthalate saturated solution;
s2, pretreating polyacrylonitrile fibers:
s2-1, weighing 299.9g of deionized water on an electronic balance, placing the weighed deionized water in a 500mL round-bottom flask, adding a stirring magnetic rotor, and stirring the mixture on a stirrer;
s2-0, inserting a pH electrode pen calibrated by S1 into a round bottom flask S2-1 filled with deionized water, and adjusting the pH value of the deionized water to 7.00 by using 0.005mol/L sodium hydroxide solution or 0.005mol/L sulfuric acid solution according to the measured value;
s2-2, measuring the wet polyacrylonitrile carbon fiber by using a filament yarn length measuring instrument in a state that the tension is 0, wherein the polyacrylonitrile carbon fiber is in a tight state when the fiber is cut off, the cut is straight and tidy, and the polyacrylonitrile fiber is placed in a round-bottom flask with the pH value of 7.00 deionized water;
s2-3, mounting a spherical condenser on the round-bottom flask, placing the round-bottom flask in a water bath heating pot, controlling the temperature of deionized water in the round-bottom flask to be 76.1 ℃, cooking fibers, and keeping the cooking time for 30 min;
s2-4, placing the cooked round-bottom flask in a water bath at 25 +/-3 ℃ for cooling, and pouring 100mL of sample solution for later use when the temperature of the mixed solution of deionized water and polyacrylonitrile carbon fibers in the flask is reduced to 25.1 ℃;
s3, polyacrylonitrile fiber pH determination: inserting the pH electrode pen calibrated in S1 into 100mL of deionized water and polyacrylonitrile carbon fiber mixed solution poured out after the treatment of S2, recording the pH value of the resin as 6.90 after the value shown by a pH meter is stable, wherein the value is the pH value of the polyacrylonitrile carbon fiber.
Example 3
A polyacrylonitrile carbon fiber pH test method comprises the following steps:
s1, calibrating a pH electrode pen:
s1-1, turning on a pH meter which is thunder magnet PHS-3C, and starting up to preheat for 15 min;
s1-2, taking out the pH electrode pen soaked in the potassium chloride solution, washing the electrode pen with deionized water for 3 times, and wiping the pH electrode pen clean with neutral filter paper;
s1-3, calibrating the pH electrode pen treated by the S1-2 in a buffer solution with the pH of 6.86 and the pH of 4, washing the calibrated pH electrode pen with deionized water for 3 times, and wiping the pH electrode pen clean with neutral filter paper; the buffer solution with the pH value of 4 is a saturated solution of potassium hydrogen phthalate;
s2, pretreating polyacrylonitrile fibers:
s2-1, weighing 300.0g of deionized water on an electronic balance, placing the deionized water in a 500mL round-bottom flask, adding a stirring magnetic rotor, and stirring the mixture on a stirrer;
s2-0, inserting a pH electrode pen calibrated by S1 into the S2-1 round bottom flask filled with deionized water, and adjusting the pH value of the deionized water to 6.98 by using 0.005mol/L sodium hydroxide solution or 0.005mol/L sulfuric acid solution according to the measured value;
s2-2, measuring the wet polyacrylonitrile carbon fiber by using a filament yarn length measuring instrument in a state that the tension is 0, wherein the polyacrylonitrile carbon fiber is in a tight state when the fiber is cut off, the cut is straight and tidy, and the polyacrylonitrile fiber is placed in a round-bottom flask with the pH value of 6.98 deionized water;
s2-3, mounting a spherical condenser on the round-bottom flask, placing the round-bottom flask in a water bath heating pot, controlling the temperature of deionized water in the round-bottom flask to be 76.0 ℃, cooking fibers, and keeping the cooking time for 30 min;
s2-4, placing the cooked round-bottom flask in a water bath at 25 +/-3 ℃ for cooling, and pouring 100mL of sample solution for later use when the temperature of the mixed solution of deionized water and polyacrylonitrile carbon fibers in the flask is reduced to 25.0 ℃;
s3, polyacrylonitrile fiber pH determination: inserting the pH electrode pen calibrated in S1 into 100mL of deionized water and polyacrylonitrile carbon fiber mixed solution poured out after the treatment of S2, recording the pH value of the resin as 6.89 after the value shown by a pH meter is stable, wherein the value is the pH value of the polyacrylonitrile carbon fiber.
The experimental results of the examples are given in the following table:
Figure BDA0002428534290000091
according to the table, the method for measuring the pH value of the polyacrylonitrile carbon fiber is simple and accurate, and the problem that the pH value of the polyacrylonitrile carbon fiber cannot be accurately measured at present is solved.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.

Claims (8)

1. A polyacrylonitrile carbon fiber pH test method is characterized by comprising the following steps:
s1, calibrating the pH electrode pen;
s2, pretreating polyacrylonitrile fibers: weighing deionized water in a flask, adding polyacrylonitrile carbon fiber for mixing, arranging a condenser on the flask, then placing the flask in a heater, controlling the temperature of the deionized water in the flask, cooking the fiber, cooling, and keeping the cold deionized water and the polyacrylonitrile carbon fiber mixed solution for later use;
s3, polyacrylonitrile fiber pH determination: inserting the pH electrode pen calibrated in the S1 into the mixed liquid of the cold deionized water and the polyacrylonitrile carbon fiber treated in the S2, and obtaining a test result of the pH value of the polyacrylonitrile carbon fiber after the test result is stable.
2. The polyacrylonitrile carbon fiber pH test method of claim 1, wherein the S1pH electrode pen calibration is specifically as follows:
s1-1, turning on a pH meter, and starting up to preheat for 10-30 min;
s1-2, taking out the pH electrode pen in the soak solution, washing the electrode pen with deionized water, and wiping the pH electrode pen clean with neutral filter paper;
s1-3, calibrating the pH electrode pen treated by the S1-2 in a buffer solution with the pH of 6.86 and the pH of 4, washing the calibrated pH electrode pen with deionized water, and wiping the pH electrode pen clean with neutral filter paper.
3. The method for testing the pH of the polyacrylonitrile carbon fiber according to claim 1, wherein the pretreatment of the S2 polyacrylonitrile fiber is as follows:
s2-1, weighing 300 +/-0.2 g of deionized water, placing the deionized water in a 500mL round-bottom flask, adding a stirring magnetic rotor, and stirring the mixture on a stirrer;
s2-2, weighing wet polyacrylonitrile carbon fibers by 3m, and placing the polyacrylonitrile fibers in a round-bottom flask filled with deionized water;
s2-3, mounting a spherical condenser on the round-bottom flask, placing the round-bottom flask in a water bath heating pot, controlling the temperature of deionized water in the round-bottom flask to be 75 +/-2 ℃, cooking fibers, and keeping the cooking time for 30 min;
and S2-4, placing the round-bottom flask after the cooking is finished in a water bath at 25 +/-3 ℃ for cooling, and pouring 100mL of sample solution for later use when the temperature of the mixture of the deionized water and the polyacrylonitrile carbon fiber in the flask is reduced to 25 +/-3 ℃.
4. The polyacrylonitrile carbon fiber pH test method of claim 2, which is characterized in that: the soak solution is saturated potassium chloride solution.
5. The method for testing the pH of polyacrylonitrile carbon fiber according to claim 3, wherein the space between S2-1 and S2-2 further comprises S2-0, a pH electrode pen calibrated by S1 is inserted into a round bottom flask of S2-1 filled with deionized water, and according to the measured value, the pH value of the deionized water is adjusted to 7.00 +/-0.03 by using a pH adjusting solution.
6. The method for testing the pH of polyacrylonitrile carbon fiber according to claim 5, wherein the pH adjusting solution is 0.005mol/L sodium hydroxide solution or 0.005mol/L sulfuric acid solution.
7. The method for testing the pH of the polyacrylonitrile carbon fiber according to claim 3, wherein when the wet polyacrylonitrile carbon fiber is measured at S2-2, the polyacrylonitrile carbon fiber is measured by a filament measuring instrument under the condition that the tension is 0, and when the fiber is sheared, the polyacrylonitrile carbon fiber is in a tight state, and the cut is straight and regular.
8. The method for testing the pH of polyacrylonitrile carbon fiber according to claim 1, wherein the pH meter used for calibrating the S1pH electrode pen is Raynaud PHS-3C.
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Application publication date: 20200602